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Designation: E 1294 – 89 (Reapproved 1999)

Standard Test Method for


Pore Size Characteristics of Membrane Filters Using
Automated Liquid Porosimeter1
This standard is issued under the fixed designation E 1294; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope 4. Significance and Use


1.1 This test method describes a procedure for measuring 4.1 This test method may be used to determine the maxi-
the pore size characteristics of membrane filters in the range of mum pore size, minimum pore size, and mean flow pore size.
approximately 0.05 to 300 µm. 4.2 The pore size distributions by flow, number, and volume
1.2 This test method uses the automated bubble point can be deduced from pressure versus flow data.
method described in ASTM Test Method F 316.
1.3 The liquid displacement technique used in this test 5. Apparatus
method depends upon the capillary rise created by surface 5.1 Source of Compressed Air up to 150 psi.
tension and uses the Washburn equation for calculating the 5.2 Automated Liquid Porosimeter.3
pore diameter. 5.3 Sample Holders.
1.4 This standard does not purport to address all of the 5.4 Metal Punch, used to cut a suitable size membrane filter
safety concerns, if any, associated with its use. It is the from the test sheet to fit the test filter holder.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 6. Reagents and Materials
bility of regulatory limitations prior to use. 6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
2. Referenced Documents all reagents shall conform to the specifications of the Commit-
2.1 ASTM Standards: tee on Analytical Reagents of the American Chemical Society
F 316 Test Method for Pore Size Characteristics of Mem- where such specifications are available.4 Other grades may be
brane Filters for Use with Aerospace Fluids2 used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
3. Summary of Test Method accuracy of the determination.
3.1 A filter wet with liquid exhibits properties similar to 6.2 Porofil.5
those of array of liquid filled capillaries (see Note). The sample 6.3 Isopropyl Alcohol.
under test is thoroughly wetted with liquid of low surface 6.4 Water.
tension and low vapor pressure and placed in a sample holder 6.5 Mineral Oil.
assembly. An increasing air pressure is applied upstream of the
sample and as successively smaller pores empty, the air flow 7. Procedure
across the sample is recorded as a function of applied pressure. 7.1 Follow the manufacturer’s operating instructions to
The point of first flow is identified as the bubble point prepare the sample to introduce to the instrument for analysis.
(maximum pore size). This continues until the smallest detect- 7.2 Establish standard sampling procedures to obtain repeat-
able pore is reached. This information is then compared with able results.
the flow rate against applied pressure response for the dry
sample. The pore size distribution is then obtained from wet 8. Operating Instructions
and dry curves. 8.1 Operating instructions shall be supplied by the manu-
facturer with every instrument. The instructions shall contain:
NOTE 1—This test method will not change the priorities of the
membrane if the test liquids are chosen to be compatible with the material
from which it is made.
3
Coulter Porometer available from Coulter Electronics, Inc., 601 W. 20th Street,
Hialeah, Florida 33010 U.S.A., has been found suitable for this purpose.
4
“Reagent Chemicals, American Chemical Society Specifications,’’ American
1
This test method is under the jurisdiction of ASTM Committee E-48 on Chemical Society, Washington DC. For suggestions on the testing of reagents no
Biotechnology and is the direct responsibility of Subcommittee E48.03 on Unit listed by the American Chemical Society, see“ Analar Standards for Laboratory U.K.
Processes and Their Control. Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”
5
Current edition approved March 31, 1989. Published May 1989. Porofil wetting liquid, available from Coulter Electronics, Inc., has been found
2
Annual Book of ASTM Standards, Vol 11.01. suitable for this purpose.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
E 1294
8.1.1 Brief instructions of the operating principles of the 11. Precision and Bias
instrument,
11.1 The precision of pore size analysis technique is not
8.1.2 Description of various systems,
easy to verify. The mathematical model chosen to relate
8.1.3 Pore size range limitations,
applied pressure to pore size is that of a right cylindrical pore.
8.1.4 Suggested maintenance procedures, and
8.1.5 Recommended spare parts. The best way to evaluate the precision is to evaluate the results
from a series of track-etched polycarbonate membranes.6 The
9. Verification manufacturer sizes them by electron microscopy, and uses
9.1 Verification of the performance of the instrument func- ASTM porosimetry and bubble point tests to validate actual
tion may be determined by using well characterized track- pore sizes.
etched polycarbonate membrane filters6 within the range of the 11.2 Precision—The reproducibility of each instrument can
instrument. be determined by repeatedly analyzing 0.1- and 10.0- µm
9.2 Interlaboratory comparisons within a particular industry polycarbonate membrane filters and determining the coefficient
should be made using these well characterized membranes. of variation. The results should not differ from the mean by
more than the following amounts:
10. Report Repeatability: (same Reproducibility: (dif-
10.1 Report the following information: Pore Size Range operator and ferent operators and
apparatus), % apparatus), %
10.1.1 Graph of raw data showing the pressure versus
percent flow. 10 µm 4 8
10.1.2 Tabulation of the raw data as well as the computed 0.1 µm 2 4

differential percent flow, cumulative percent flow, differential Since the change in pore size per unit change in applied
number percent, and cumulative number percent. pressure is greatest at large pore sizes and diminished hyper-
10.1.3 Graphs of differential and cumulative flow as well as
bolically, repeatability and reproducibility increase accordingly
number distributions plotted as pore size versus percent flow or
with applied pressure.
percent number.
11.3 Bias—The bias between two different instruments can
be determined by comparing the mean flow pore sizes.
6
Polycarbonate membrane filters, available from Nucleopore Corp., 7035
Commerce Circle, Pleasanton, CA 94566, have been found suitable for this purpose.

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